Archives of Environmental Protection PL ISSN 2083-4772

Vol. 43 no. 1 pp. 20–26 DOI 10.1515/aep-2017-0003

© Copyright by Polish Academy of Sciences

and Institute of Environmental Engineering of the Polish Academy of Sciences,
Zabrze, Poland 2017

Removal efficiency of anionic surfactants

from water during UVC photolysis and advanced oxidation
process in H2O2/UVC system
Francisco Ríos1, Magdalena Olak-Kucharczyk2, Marta Gmurek2, Stanisław Ledakowicz2*
1 
Department of Chemical Engineering, Spain
University of Granada
2 
Lodz University of Technology, Poland
Department of Bioprocess Engineering

* Corresponding author’s e-mail: stanislaw.ledakowicz@p.lodz.pl

Keywords: advanced oxidation process, anionic surfactants, ether carboxylic derivate, H2O2/UVC system, linear
alkyl benzene sulfonate, UVC photolysis.

Abstract: Surfactants after their use are discharged into aquatic ecosystems. These compounds may be harmful to
fauna and flora in surface waters or can be toxic for microorganisms of the activated sludge or biofilm in WWTP.
In order to determine effectiveness of different advanced oxidation processes on the degradation of surfactants, in
this study the degradation of anionic surfactants in aqueous solution using photolysis by 254 nm irradiation and by
advanced oxidation process in a H2O2/UVC system was investigated. Two representatives of anionic surfactants,
linear alkyl benzene sulphonate (LAS-R11–14) and ether carboxylic derivate (EC-R12–14E10) were tested. The influence
of pH, initial surfactant concentration and dose of hydrogen peroxide on the degradation was also studied. Results
show outstanding effectiveness of the H2O2/UVC system in the removal of surfactant from aqueous solutions.

Introduction produces foams, which leads to the perturbation of treatment

Surfactants are a wide group of chemical compounds which
have a large number of applications in household cleaning
detergents, personal-care products, textiles, paints, polymers,
pesticides, pharmaceuticals, mining, oil recovery, and the
pulp and paper industries (Fernández-Serrano et al. 2014,
Zgola-Grześkowiak et al. 2015, Jurado et al. 2013). Moreover,
biosurfactants such as saponin, tannin and rhamnolipids JBR
515 and 425 can be applied for heavy metals removal from
immobilized activated sludge (Kuczajowska-Zadrożna et al.
2015). After their use, surfactant residues and their degradation
products are discharged into aquatic ecosystems in treated or
untreated wastewaters, and enter in various environmental
compartments such as surface waters, sediments and biota
(Ying 2006). Recent studies have demonstrated the persistence
and accumulation of surfactants and their biodegradation
products in the environment (Sanz et al. 2013, Cserháti et al.
2002, Petrovic et al. 2002, Robert-Peillard et al. 2015). Several
of these compounds may be harmful to fauna and flora in
surface waters. For example, surfactants may cause acute and
chronic effects on sensitive organisms, such as crustaceans and
fish (Roberts and Marshall 1995, Ferrara et al. 2005). Moreover,
they affect the growth, motility and photosynthetic ability of
algae (Rebello et al. 2014). The presence of high concentrations
of surfactants in biologic stations of WWTP inhibits aerobic
microorganisms, is toxic to anaerobic microorganisms, and
process (Aloui et al. 2009, Bozkurt and Sanin 2014).
According to the European Committee of Organic
Surfactants and their Intermediates, the total quantity of
surfactants excluding soap produced in Western Europe in 2013
was equal to 2.98 million tons (CESIO 2014). It is predicted
that the surfactant market will grow with a compound annual
growth rate (CAGR) of 6.19% until 2017 (Markets 2013).
The universality of application of these compounds leads to
their presence in water environment. The concentration of
LAS-R11–14 in raw sewage ranged from 1 to 15 mg dm-3 while
in surface water LAS-R11–14 were detected below 0.05 mg dm-3
(HERA 2013). However, the concentration of this compound in
industrial wastewater as well as in laundry sewage was found
to be about 200 mg dm-3 (Han 2013) and up to 1024 mg dm-3
(Braga 2011), respectively. Therefore, it is required finding the
proper methods of their degradation.
Biodegradation is the cheapest method of the pollutants
degradation (Chidambara and Quen 2005), however, in many
cases surfactants solutions are toxic for microorganisms of the
activated sludge or biofilm (Ledakowicz et al. 2005) causing
strong inhibition on dehydrogenase activity of activated sludge
biomass (Liwarska-Bizukojc and Bizukojc 2008). Furthermore,
some surfactant molecules are not readily biodegradable and
relatively high residuals as well partially degraded products are
found in the treated effluents and receiving waters (Ying 2006).
Therefore, a more efficient option for highly concentrated
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 Removal efficiency of anionic surfactants from water during UVC photolysis and advanced oxidation process...
surfactant effluents could be the coupling of advanced
oxidation and the biological process that could reduce the final
concentration of contaminant in the WWTP outlet (Sanz et al.
2013, Lechuga et al. 2014).
Advanced oxidation processes (AOPs) have been
extensively studied for the removal of recalcitrant xenobiotic
compounds from water and wastewater (Luo et al. 2014).
These processes have several advantages over conventional
chemical oxidation using potassium permanganate or chlorine,
for example higher oxidation potential and no production of
potentially carcinogenic chlorinated by-products. Moreover,
the oxidants used in AOPs are in situ generated and not
persistent, so they do not affect the biological treatment
processes (Ikehata and El-Din 2004). The anionic surfactant
LAS-R11–14 is relatively well degraded by some AOPs including
ozonation, Fenton, photo-Fenton and H2O2/UV processes
(Sanz et al. 2013, Pagano et al. 2008, Lechuga et al. 2014).
In recent years, study on effective removal of LAS-R11–14
and other important non-ionic surfactants is becoming more
and more active topic. Some studies, such as this published
by Sanz et al. (2013), demonstrated the influence of reaction
temperature on the degradation of LAS using a H2O2/UV
system. Pagano et al. (2008) studied the oxidation of alcohol
ethoxylates and alkylpehol ethoxylates by Fenton and
H2O2/UV processes, while Lechuga et al. (2014) indicated
that the removal of LAS is increased by the consecutive use
of ozonation and biodegradation. However, the degradation of
new families of surfactants by AOPs, such as ether carboxylic
derivates remains unstudied.
In order to contribute to increasing the information
concerning the effectiveness of different AOPs, the present
investigation was specifically aimed at the degradation of
two different anionic surfactants by direct photolysis and
advanced oxidation in H2O2/UVC system. The influence of
various parameters in the degradation (pH, initial surfactant
concentration and dose of hydrogen peroxide) was also studied.
Methods
Two anionic surfactants were used in this study: linear alkyl
benzene sulfonate (LAS-R11–14), supplied by Petresa (Madrid,
Spain), and ether carboxylic derivate (EC-R12–14E10) supplied
by Kao Corporation S.A. (Tokyo, Japan). Table 1 shows the
structure, the percentage of active matter and the critical
micelle concentration (CMC) of the surfactants tested. The
initial surfactants concentrations used ranged from 9.3 to
60.0 mg dm-3 and from 6.4 to 89.3 mg dm-3 for LAS-R11–14
and EC-R12–14E10, respectively. These concentrations were
chosen in order to study the degradation of surfactants above
Table 1. Description of the surfactants used (R: alkyl-chain length, n: degree of ethoxylation, X=H+ or Na)
Surfactant Linear alkyl benzene
Abbreviation LAS-R11–14
Structure R-CH-(CH3)(C6H4)-SO3 Na-
% Active Matter 46.8a
CMC, mg dm-3 25.5b
a
Supplied by the manufacturer
b
(Lechuga et al. 2013)
21
and below the CMC. The used concentration of hydrogen
peroxide (30%) (POCH, Poland) ranged from 1×10-2 mol dm-3
to 1×10-1 mol dm-3.
All the solutions used in the experiments were prepared in
distilled water treated in Millipore Milli-Q Plus System and the
pH of the solutions was adjusted by a phosphate buffer (H3PO4,
KH2PO4, Na2HPO4, NaOH, all p.a., POCh, Poland) in the range
from 2 to 12.
For both process: UVC photolysis and the H2O2/UVC
system, low-pressure lamps (Luzchem) emitting mainly at
the wavelength λ = 254 nm were applied. The tested solutions
were irradiated in a merry-go-round device with quartz test
tubes (volume: 10 cm3, average optical path length: 0.85 cm),
placed between two exposure panels, each of them consisting
of three 7.2 W lamps. The samples were irradiated for 120 min
in the case of UVC photolysis and for 4 min when the
H2O2/UV system was used. In the case of H2O2/UV system,
degradation experiments were additionally performed in the
presence of hydroxyl radicals scavenger. In these studies
1×10-1 mol dm-3 tert-butanol (Fluka) was used. The experiments
were performed at room temperature equal to 22ºC.
The surfactant degradation was monitored by means of the
residual-surfactant concentration over time using a colorimetric
method in which the absorbance is directly proportional to the
surfactant concentration. The method is based on the formation
of the ionic-pair anionic surfactant-methylene blue (Jurado et
al. 2006). For spectrophotometric measurements, 5×10-3 dm3
of sample placed in 1×10-2 dm3 glass vials were made alkaline
to pH 10.0 by adding 2×10-4 dm3 of 5×10-2 mol dm-3 sodium
tetraborate, pH 10.5, and then 10-4 dm3 of methylene blue 1 g dm-3
stabilized was added. Finally, 4×10-3 dm3 of chloroform was
added and, after stirring and 5-min wait, the absorbance at
650 nm was measured. This method allows to measure the
concentration of LAS-R11–14 and EC-R12–14E10 with a limit of
detection of 0.05 mg dm-3.
The initial reaction rates were calculated by differentiating
exponential curve that fitted experimental points (C, t) at the
correlation factor higher than 0.97.
Results and discussion
In the beginning, the possibility of surfactants degradation
during exposure to UVC radiation was tested.
Fig. 1 presents absorption spectra of the tested substances
at different pH and the emission spectrum of the UV lamps.
LAS-R11–14 molecules absorb radiation with maximum at
224 nm, while EC-R12–14E10 very poorly absorbs UVC radiation.
The investigated compounds were irradiated for
120 minutes and the influence of their initial concentration and
Ether carboxylic derivative
EC-R12–14E10
+
R-(CH2-CH2O)n-O-CH2-COO-X
94.0a
69.0b
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22 F. Ríos, M. Olak-Kucharczyk, M. Gmurek, S. Ledakowicz

pH were studied. Fig. 2 shows changes of relative surfactant
concentration versus radiation dose (E). The degradation
of investigated compounds during photolysis by 254 nm
irradiation occurs slowly and is a highly energy-consuming
process. The use of radiation dose of 57.2 kJ m-2 results in
about 10% reduction of initial surfactants concentration
(Fig. 2). While, the UV disinfection dose usually applied for
tap water treatment is equal to 0.4 kJ m-2 (Canonica et al.
2008), therefore it is no possible to remove these compounds
during disinfection process.
In the case of EC-R12–14E10, the photolysis occurs
the fastest in neutral pH (Fig. 3A), while the increase in
alkalinity practically does not influence the reaction rate of
LAS-R11–14 photolysis (Fig. 3A). An increase in the initial
concentration caused increase of EC-R12–14E10 reaction
rate (Fig. 3B), and did not accelerate the LAS-R11–14
photodegradation (Fig. 3B).
The addition of hydrogen peroxide to the reaction
solution resulted in a significant acceleration of degradation
process (Fig. 2). A 10-fold lower radiation dose (5.72 kJ m-2)
than mentioned above for photolysis allows for 60% reduction
of initial LAS-R11–14 concentration (Fig. 2A) and about 50%
reduction of initial EC-R12–14E10 concentration (Fig. 2B).
Pagano et al. (2008) also found high removal rates of
surfactants: alcohol ethoxylates and alkylphenol ethoxylates
using the H2O2/UV process.
The degradation in the H2O2/UV system requires
establishing of an optimal hydrogen peroxide concentration,

1.6 1.6

1.4 1.4

Emission of the lamp, a.u

EC-R12-14E10 pH 2
1.2 EC-R12-14E10 pH 7 1.2
EC-R12-14E10 pH 12
Absorbance, a.u

1.0 1.0
LAS: R11-14 pH 2

0.8 LAS: R11-14 pH 7 0.8

LAS: R11-14 pH 12
0.6 UVC LP 0.6

0.4 0.4

0.2 0.2

0.0 0.0
200 250 300 350 400
λ, nm

Fig. 1. Absortion spectra of LAS-R11–14 (A) (C0=45 mg dm-3) and EC-R12–14E10 (B) (C0=26 mg dm-3) at pH=2, 7
and 12, overlayed against emission spectra of UVC lamps used in experiments

A) B)

1.0 1.0

0.9
0.9

0.8
0.8
0.7
C/C0
C/C0

UVC 0.7
UVC
0.6 UVC/H2O2 UVC/H2O2
UVC/H2O2 + t-BuOH UVC/H2O2 + t-BuOH 0.6
0.5

0.4 0.5

0.3 0.4
0 10 20 30 40 50 60 0 10 20 30 40 50 60
-2 -2
E, kJ m E, kJ m

Fig. 2. Changes of relative LAS-R11–14 (A) (C0=45 mg dm-3, CH2O2=3×10-2 mol dm-3, CtBuOH=1×10-1 mol dm-3, pH=7,
E0=10.6×10-6 einstein dm-3 s-1) and EC-R12–14E10 (B) (C0=26 mg dm-3, CH2O2=3×10-2 mol dm-3, CtBuOH=1×10-1 mol dm-3,
pH=7, E0=10.6×10-6 einstein dm-3 s-1) concentration during the photolysis and advanced oxidation
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 Removal efficiency of anionic surfactants from water during UVC photolysis and advanced oxidation process... 23

i.e. when the H2O2 photolysis produces plenty of ●OH radicals was strongly inhibited, which is mainly connected with the
and their consumption by hydrogen peroxide is negligible. hydrogen peroxide dissociation (1) (pKa=11.6 (Hoigne 1998)).
The highest reaction rate of the surfactants degradation The anions formed in this reaction have a much higher molar
was attained at H2O2 concentration of 3×10-2 mol dm-3, absorption coefficient in comparison to hydrogen peroxide
as shown in Fig. 4. This optimal H2O2 concentration was (ε254nm=240 M-1cm-1 (Legrini et al. 1993), ε254nm=18.6 M-1 cm-1
chosen to evaluate the influence of other parameters on (Nicole et al. 1990)), and can react both with H2O2 (2) and ●OH
the advanced oxidation of the investigated surfactants in (3) radicals leading to reduction of ●OH radicals concentration
H2O2/UV system. in the reaction mixture.
The results of advanced oxidation in H2O2/UV system
at various pH of reaction solutions are presented in Fig. 5. H2O2 + H2O → H3O+ + HO2- (1)
In the case of LAS-R11–14 the process occurs with a similar
efficiency at neutral and acidic conditions (Fig. 5A), whereas H2O2 + HO2- → H2O + O2 + ●OH (2)
for EC-R12–14E10 it is the most effective at pH 7 (Fig. 5B). In
alkaline solutions degradation of investigated compounds ●
OH + HO2- → H2O + O2● - (3)

A) B)
0.20 0.20

0.18 LAS-R11-14 0.18

0.16 EC-R12-14E10 0.16

0.14 0.14

0.12 0.12
-3 -1

-3 -1
r0, mg dm s

r0, mg dm s
0.10 0.10

0.08 0.08

0.06 0.06

0.04 0.04

0.02 0.02

0.00 0.00

2 4 6 8 10 12 0 20 40 60 80 100
pH C0, mg dm
-3

Fig. 3. Influence of pH (A) (LAS: R11–14: C0=46 mg dm-3, E0=10.6×10-6 einstein dm-3 s-1; EC-R12–14E10: C0=30 mg dm-3,
E0=10.6×10-6 einstein dm-3 s-1) and initial surfactant concentration (B) (E0=10.6×10-6 einstein dm-3 s-1, pH=7)
on initial reaction rate

0.8

0.7 LAS-R11-14
EC-R12-14E10
0.6

0.5
-3 -1
r0, mg dm s

0.4

0.3

0.2

0.1

0.0
0.00 0.02 0.04 0.06 0.08 0.10 0.12
-3
CH2O2, mol dm

Fig. 4. Dependence of initial reaction rate on hydrogen peroxide concentration (LAS-R11–14: C0=50 mg dm-3,
pH=7, E0=10.6×10-6 einstein dm-3 s-1; EC-R12–14E10: C0=40 mg dm-3, pH=7, E0=10.6×10-6 einstein dm-3 s-1)
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24 F. Ríos, M. Olak-Kucharczyk, M. Gmurek, S. Ledakowicz

The surfactant degradation at four different initial
concentrations was studied (Fig. 6). In the case of LAS-R11–14,
there is an optimal concentration (26 mg dm-3) above which
degradation process slowed down (Fig. 6A), what can be
explained by the advantage of this compounds over H2O2 in
the competition of photons and domination of direct photolysis
of LAS-R11–14. CMC of LAS-R11–14 is equal to 25.5 mg dm-3
(Table 1) and the optimal concentration coincides with this
value, i.e. when the solubilization of the surfactant molecules
takes place in micelles. However, at concentrations above the
CMC the degradation does not occur faster, and the percentage of
degradation is lower (Fig. 6A). In addition, this process slowed
down when the LAS-R11–14 concentration was below CMC due
to the fact that the molecules of surfactants were mainly in the
water-air interface and access to them was more difficult.
In the degradation process of EC-R12–14E10, increase of
initial concentration leads to the acceleration of reaction
efficiency and reducing the energy input (Fig. 6B). During
advanced oxidation of EC-R12–14E10, 40% reduction of the
initial concentration equal to 7.5 mg dm-3 was achieved
by using radiation dose of 3.81 kJ m-2. About 6-fold higher
initial concentration of these compounds results in 4-fold
decreases of radiation dose which is needed to achieve the
above degradation degree (Fig. 6B). The influence of CMC
on advanced oxiadation of EC-R12–14E10, cannot be studied
because its initial concentration was below CMC in all cases.

A) B)

1.0 1.0

0.8 0.8

0.6 0.6

C/C0
C/C0

0.4 0.4

pH 2 pH 2
0.2 pH 7 0.2
pH 7
pH 12 pH 12
0.0 0.0
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
-2
E, kJ m E, kJ m
-2

Fig. 5. Changes of relative LAS-R11–14 (A) (C0=54 mg dm-3, CH2O2=3×10-2mol dm-3, E0=10.6×10-6 einstein dm-3 s-1)
and EC-R12–14E10 (B) (C0=26 mg dm-3, CH2O2=3 ×10-2 mol dm-3, E0=10.6×10-6 einstein dm-3 s-1) concentration during
advanced oxidation in various pH values

A) B)
1.0 1.0
-3 -3
15 mg dm 7.5 mg dm
0.9 -3 -3
26 mg dm 26.6 mg dm
0.8 43 mg dm
-3
28 mg dm
-3 0.8
-3 -3
0.7 60 mg dm 43.8 mg dm

0.6 0.6
C/C0
C/C0

0.5
0.4 0.4

0.3
0.2 0.2

0.1
0.0
0.0
0 1 2 3 4 5 6 7 8 0 1 2 3 4 5 6 7 8
-2 -2
E, kJ m E, kJ m

Fig. 6. Changes of relative LAS-R11–14 (A) (CH2O2=3×10-2 mol dm-3, pH=7, E0=10.6×10-6 einstein dm-3 s-1)
and EC-R12–14E10 (B) (CH2O2=3×10-2 mol dm-3, pH=7, E0=10.6×10-6 einstein dm-3 s-1) concentration during
advanced oxidation for various intial concetrantion of surfactant Unauthenticated
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 Removal efficiency of anionic surfactants from water during UVC photolysis and advanced oxidation process...
In addition, surfactant degradation was studied in the
presence of hydroxyl radical scavengers (Fig. 2). The influence
of tert-butanol on the reaction run was investigated. For both
surfactants, the reaction is not inhibited to the direct photolysis
level, what may suggest that an additional reaction (“third
pathway”) occurs. Similar situation was observed during
butylparaben (Błędzka et al. 2010) and fluorene (Ledakowicz
et al. 1999) degradation in H2O2/UV system.
Conclusions
The studies performed on degradation of two surfactants:
linear alkyl benzene sulphonate and ether carboxylic derivate
exposed to UVC irradiation in aqueous solutions with and
without addition of hydrogen peroxide enable us to draw the
following conclusions.
The photolysis of EC-R12–14E10 occurs the fastest in neutral
pH, while the increase in alkalinity practically does not
influence reaction rate of LAS-R11–14 photolysis.
An increase in the initial concentration of surfactants
caused increase of photolysis rate.
Advanced oxidation of EC-R12–14E10 is the most effective
at pH 7, whereas for LAS-R11–14 it occurs with a similar
efficiency at neutral and acidic conditions. However, for both
investigated compounds this process was strongly inhibited in
alkaline solutions.
The highest degradation rate of surfactants in H2O2/UV
system was attained at H2O2 concentration of 3×10-2 mol dm-3.
Increase of EC-R12–14E10 initial concentration leads to
the acceleration of advanced oxidation, while in the case of
LAS-R11–14, there is an optimal concentration above which
degradation process slowed down.
Advanced oxidation process in a H2O2/UV system
represents an effective method to degrade surfactants. This
technique has advantages over using photolysis alone:
degradation is a faster and less energy-consuming process.
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Efektywność usuwania surfaktantów anionowych z wody przy zastosowaniu

promieniowania UVC i zaawansowanego utleniania w układzie H2O2/UVC

Streszczenie: Surfaktanty, podobnie jak większość tego typu substancji chemicznych, po wykorzystaniu trafiają
do środowiska wodnego. Związki te mogą stwarzać zagrożenie dla flory i fauny zasiedlającej wody powierzch-
niowe, jak również mogą działać toksycznie na mikroorganizmy znajdujące się w osadzie czynnym w oczyszc-
zalniach ścieków.
W niniejszej pracy przedstawiono wyniki badań degradacji wybranych surfaktantów anionowych w środowisku
wodnym przy zastosowaniu promieniowania UVC i zaawansowanego utleniania w układzie H2O2/UVC. Zbadano
wpływ następujących parametrów reakcyjnych: odczyn środowiska reakcyjnego, początkowego stężenia obiek-
tów badań i nadtlenku wodoru na szybkość degradacji surfaktantów. Uzyskane w toku prac badawczych wyniki
potwierdzają wysoką skuteczność zaawansowanego utleniania w układzie H2O2/UVC w usuwaniu badanych surfak-
tantów ze środowiska wodnego, które jest procesem znacznie efektywniejszym w porównaniu do procesu fotolizy.

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